US9984874B2 - Method of producing transition metal dichalcogenide layer - Google Patents
Method of producing transition metal dichalcogenide layer Download PDFInfo
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- US9984874B2 US9984874B2 US15/039,407 US201415039407A US9984874B2 US 9984874 B2 US9984874 B2 US 9984874B2 US 201415039407 A US201415039407 A US 201415039407A US 9984874 B2 US9984874 B2 US 9984874B2
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- transition metal
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- metal dichalcogenide
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- H01L21/02664—Aftertreatments
Definitions
- the invention relates to methods of producing transition metal dichalcogenide layers on a substrate.
- the invention relates in particular to methods of producing a limited number of layers, for instance less than seven layers of transition metal dichalcogenides on a relatively large substrate.
- a next generation of materials are two-dimensional materials such as graphene, which is in fact a two-dimensional sheet of carbon atoms arranged in hexagonal rings.
- Graphene offers extremely high carrier mobilities but has basically no bandgap. Measures to open up the bandgap (‘chemical functionalization’) are known but deteriorate at the same time its mobility, hence graphene is losing much of its attraction as alternative MOS channel material.
- TMDCs transition metal dichalcogenides
- MX 2 a transition metal such as e.g. W or Mo
- X a chalcogen, i.e. a non-metal of the oxygen group, such as e.g. S, Se or Te.
- TMDCs have found interest as alternative candidate 2D materials due to the fact that they have a natural finite band gap, in contrast to graphene.
- TMDC materials especially for instance MoS 2
- lubricants have properties very similar to graphite.
- they are composed of a layered material with strong in-plane bonding and weak out-of plane interactions (the layers are only weakly bonded by van der Waals forces), such that individual layers can easily move with respect to each other and in this way reduce friction between moving parts. It is known e.g.
- MX 2 is composed of a single metal layer sandwiched between two chalcogen atomic layers which are each arranged in a 2D hexagonal honeycomb structure, as illustrated in FIG. 1 .
- a top view is shown, and on the right of FIG.
- a side view is shown of a stack consisting of four tri-atomic layers.
- MX 2 material Two polymorphs of MoS 2 are the so-called 2H and 3R symmetries characterized by a different stacking of the monolayers, as illustrated in FIG. 2 .
- the 2H is the more stable one.
- the bandgap evolves from indirect to direct, which makes it also interesting for optical applications in integrated circuits.
- MX 2 layers in relatively large areas and/or with the desired orientation (e.g. substantially parallel to the substrate) so as to make them fit for integration into high-volume semiconductor manufacturing on e.g. 300 or 450 mm semiconductor substrates, e.g. silicon wafers.
- the best known method for making device-quality MX 2 is the exfoliation technique applied on naturally occurring mono-crystals of MX 2 . This results in tiny flakes of only few micrometer size.
- Many approaches have been studied to produce samples of layered MX 2 , but as far as known to the inventors, so far none of them resulted in techniques suitable for manufacturing on industrial scale. Industrial alternatives to exfoliation are deposition methods.
- PVD physical and chemical vapor deposition
- molecular beam epitaxy Other approaches are based on consecutively depositing the metal or metal oxide (e.g. Mo or MoO 3 ) by evaporation followed by a chalcogenidation reaction in e.g. X or H 2 X vapor. As these reactions proceed typically at very high temperature, e.g. in the order of 650-1000° C., and/or require long annealing times, e.g. in the order of several hours, they are not very efficient. Moreover, often they do not result in large area flat deposits with the desired horizontal (i.e. parallel to the substrate surface) layering.
- the metal or metal oxide e.g. Mo or MoO 3
- CVD chemical vapor transport
- ALD atomic layer deposition
- a “layer of a 2D transition metal dichalcogenide” is made of a tri-atomic layer structure consisting of a single metal layer (or plane) sandwiched between two chalcogen atomic layers (or planes), and is also referred to herein as a “monolayer” of MX 2 material.
- the present invention provides a method of producing at least one transition metal dichalcogenide layer on a substrate.
- the method comprises:
- the ALD deposition may be thermal ALD deposition.
- the ALD deposition may be plasma enhanced ALD deposition (PEALD).
- the substrate may be a semiconductor substrate, such as for instance a silicon substrate.
- the substrate may comprise at least one layer of dielectric material, which could be obtained for example by deposition, or by oxidation of the semiconductor material, the present invention not being limited thereto.
- the dielectric layer may comprise for example an oxide, for example an oxide layer.
- the substrate may be a SOI substrate, where a semiconductor layer is provided on top of a dielectric layer, on top of a substrate.
- an oxide layer dielectric layer
- the thin layer on top of the dielectric layer may comprise few monolayers of material, for example 2 monolayers, for example a single monolayer, and it may act as a sacrificial layer during ALD.
- the thickness of the layer of material on top of the dielectric layer may control the ALD process. It is an advantage of a method according to embodiments of the present invention that the need for a catalyst comprising Zn during ALD initiation can be avoided, which allows obtaining highly pure deposited films.
- a method according to embodiments of the present invention may include a step of functionalization of the substrate surface before depositing the transition metal dichalcogenide layer.
- Functionalization may for example be performed with reagents such as H 2 S, or silicon- or boron-hydrogen compounds (e.g. silane (SiH 4 ), disilane (Si 2 H 6 ), trisilane (Si 3 H 8 ), diborane (B 2 H 6 )), or a combination thereof, for example applied by plasma pulses.
- reagents such as H 2 S, or silicon- or boron-hydrogen compounds (e.g. silane (SiH 4 ), disilane (Si 2 H 6 ), trisilane (Si 3 H 8 ), diborane (B 2 H 6 )), or a combination thereof, for example applied by plasma pulses.
- functionalization may be performed by means of an O 3 oxidation.
- functionalization may be performed on the surface of the substrate, in particular for instance on a sacrificial layer of the substrate, or on a dielectric top layer of the substrate.
- the inventors have found that, by functionalizing the surface, e.g. sulphidizing the surface or treating it with ozone before depositing the transition metal dichalcogenide layer by the ALD technique, the need for a catalyst comprising Zn during the ALD initiation can be avoided, and hence a high purity film can be preserved, or in other words, the contamination of the transition metal dichalcogenide layer by unwanted chemical elements (such as e.g. carbon and/or Zn) can be reduced or even eliminated.
- functionalizing the surface e.g. sulphidizing the surface or treating it with ozone before depositing the transition metal dichalcogenide layer by the ALD technique
- the need for a catalyst comprising Zn during the ALD initiation can be avoided, and hence a high purity film can be preserved, or in other words, the contamination of the transition metal dichalcogenide layer by unwanted chemical elements (such as e.g. carbon and/or Zn) can be reduced or even eliminated.
- a method according to embodiments of the present invention allows excellent film thickness control and uniformity. In particular, it allows to deposit for example only a single transition metal dichalcogenide monolayer, or only two transition metal dichalcogenide monolayers.
- the method is particularly suitable for producing channels comprising, or consisting of, transition metal dichalcogenides, as part of a transistor or TFET.
- depositing the transition metal dichalcogenide layer by using ALD deposition may comprise using thermal ALD, or may comprise using plasma-enhanced ALD (PEALD), wherein H 2 X plasma may be used.
- the plasma can be formed in pure H 2 X or in H 2 X gas mixtures, either dilutions with inert gas (He or Ar) or H 2 /H 2 X gas mixtures can be used.
- PEALD may advantageously be performed after functionalization of the substrate, for example after functionalization comprising silicon- or boron-hydrogen reagents, although the present invention is not limited thereto and PEALD may be applied after sulphidizing, or after any other type of functionalization, or even directly on the obtained substrate, omitting the functionalization step.
- depositing the transition metal dichalcogenide layer by using ALD deposition may be performed at a deposition temperature in the range of 250° C. to 450° C.
- ALD reactors are very well accepted in nowadays state-of-the-art semiconductor manufacturing.
- a method according to embodiments of the present invention may furthermore comprise, before functionalizing the surface, removing a native oxide from the surface.
- removing a native oxide from the surface for instance embodiments where a dielectric layer such as an Al 2 O 3 layer is deposited on the substrate surface in order to protect the underlying substrate from etching, such removal of native oxide is not required.
- removing native oxide may comprise HF/H 2 O dipping the substrate. In particular embodiments of the present invention, this may leave approximately 10% of a monolayer of O on the surface, which is sufficient to expose the (111) Si surface for epitaxial seeding.
- Removing native oxide may furthermore comprise H 2 baking of the substrate during at least five minutes at a temperature in the range of 700° C. to 800° C.
- functionalizing the surface may comprise an O 3 oxidation at 40° C. to 80° C. during 200 to 1000 msec. During such controlled O 3 oxidation, OH groups are provided to functionalize the surface.
- functionalizing the substrate may comprise annealing the substrate with H 2 S at a temperature in the range of 300° C. to 550° C. during a period ranging from 1 to 40 minutes. During such operation, SH groups are provided to functionalize the surface.
- the metal of the metal halide precursor may be selected from the group consisting of Mo and W, and the chalcogen of the chalcogen source may be selected from the group consisting of S, Se and Te.
- MoS 2 and WSe 2 are advantageous because they have the highest mobilities. MoS 2 is particularly advantageous since:
- the substrate used in a method according to embodiments of the present invention may be a (111) oriented semiconductor substrate, or a substrate having a surface which is suitable for epitaxial seeding of a transition metal dichalcogenide layer.
- a semiconductor substrate e.g. a silicon substrate
- in the (111) orientation as seeding layer for epitaxial growth of the transition metal dichalcogenides layer to be deposited, as this allows tight orientation control of this layer. More in particular, it allows to better control the angle between the plane containing the atomic metal layer and the surface of the substrate.
- This provides a.o. the advantages of 1) flat transition metal dichalcogenide layer (basal plane parallel to wafer surface), and 2) in principle no limitations to the area of the transition metal dichalcogenide layer (like in the exfoliation case) on large area wafers.
- (111) Si wafers are not conventional for CMOS, such wafers are commercially available.
- the present invention provides a method of producing at least two transition metal dichalcogenide materials on a substrate.
- the method comprises the steps of:
- first metal halide precursor is different from the second metal halide precursor and/or the first chalcogen source is different from the second chalcogen source.
- the first and second metals and chalcogenides may be mixed inside the monolayer itself, such as for instance by forming a layer of Mo (1-x) W x S 2(1-y) Se 2y .
- heterogeneous combinations of homogeneous monolayers e.g. MoS 2 on top of WSe 2 may be made.
- metal dichalcogenides e.g. MoS 2 /WS 2
- first layer consisting of a first predefined number N1 of first monolayers (where N1 is an integer value in the range of 1 to 5
- second layer consisting of a second predefined number N2 of second monolayers (where N2 is an integer in the range of 1 to 5
- the stack of all monolayers may be arranged as a lower part of the N1 first monolayers and an upper part of the N2 second monolayers, or as interleaved, e.g. alternating, first and second layers.
- MoF 6 and H 2 S for depositing the first layer, and MoF 6 and H 2 Se for the second layer, or vice versa
- one can make a mixed channel layer MoS 2 /MoSe 2 in well-controlled ratios, e.g. predefined ratios.
- Such a method allows to make semiconductor structures with channels made of different materials in predefined ratios. This allows bandgap engineering of the deposited materials.
- MX 2 metal dichalcogenide
- the use of such mixtures allows tuning of electronic or optoelectronic properties of the devices manufactured with these layers.
- FIG. 1 shows a crystalline structure of MoS 2 in 2H configuration, in top view (left) and side view (right). The right part of the figure will be referred to as a stack of four monolayers.
- FIG. 2 shows crystalline structures of transition metal dichalcogenides MX 2 in 2H, 3R and 1T configuration, where X is an element selected from the group of S, Se and Te, and M is a transition metal selected from the group of W and Mo, ‘a’ is the unit cell parameter of the trigonal base plane, and ‘c’ is the inter-layer distance.
- FIG. 3 illustrates a method according to embodiments of the present invention.
- FIG. 4 illustrates a method according to particular embodiments of the present invention, where the substrate is a semiconductor substrate.
- FIG. 5( a ) illustrates the thickness of an S-layer deposited on a substrate after 20 minutes, in function of temperature.
- FIG. 5( b ) illustrates the number of S atoms per unit area (cm 2 ) deposited on a substrate after 20 minutes, in function of temperature.
- FIG. 5( c ) illustrates the thickness of the S layer deposited at a temperature of 500° C., in function of time.
- FIG. 5( d ) illustrates the number of S atoms per unit area (cm 2 ) deposited at a temperature of 500°, in function of time.
- FIG. 6 illustrates a method according to particular embodiments of the present invention, where the substrate comprises a dielectric top layer.
- FIG. 1 illustrates a stack of four monolayers, each being a two-dimensional transition metal dichalcogenide layer, comprising a transition metal layer sandwiched in between two chalcogenide layers.
- atomic layer deposition is a known technique for depositing two-dimensional (2D) transition metal dichalcogenides (MX 2 ) on a semiconductor, for instance silicon, substrate.
- MX 2 transition metal dichalcogenides
- Suitable metal halide precursors are e.g. the metal hexafluorides, such as WF 6 , MoF 6 .
- WF 6 is a well-known gas in semiconductor manufacturing, used in dry etch processes.
- MoF 6 is a solid with melting point of about 17.5° C., and hence is liquid at room temperature (25° C.). They are commercially available.
- the present invention is not limited thereto, and other materials (e. g. comprising other halogens such as Cl) may be used.
- An ALD process in embodiments of the present invention may be a thermal ALD process or a plasma enhanced ALD process.
- a general ALD process different precursors are injected into the reactor in consecutive pulses, and separated by purge steps with an inert purge gas. The assembly of pulses and purges is called a unit deposition cycle.
- the precursor In every precursor pulse, the precursor adsorbs on the surface until saturation.
- a thermal ALD process the precursors will react with the surface and form a chemical bond, activated by the temperature. In this case, heat is applied to initiate a chemical reaction between the surface and the adsorbent, so as to facilitate surface reactions which allow for the formation of thin films in a stepwise fashion.
- a plasma enhanced ALD process is an ALD process including a plasma enhancement step rather than a thermal activation.
- reactions are initiated by using energy from a plasma.
- the plasma enhancement can take place during one of the precursor pulses, or after any of the precursor pulses (metal halide precursor and chalcogen source).
- Suitable chalcogen sources are H 2 X, e.g. H 2 S, H 2 Se, H 2 Te, all gaseous at room temperature and also well known in semiconductor manufacturing. They are also commercially available.
- Typical overall half-reaction schemes for ALD deposition of WX 2 where X ⁇ S or Se or Te, are as follows: 2*+H 2 X ⁇ X H+H a. X H+WF 6 ⁇ X WF x +HF b. with * denoting an active surface site and X H an XH group connected to a surface site. HF is an extremely effective leaving group. As such, these precursors allow growth of very pure MX 2 films without substantial contamination such as e.g. by carbon, which can be found when using metalorganic precursors.
- the inventors of the present invention have discovered that the undesired deposition of Zn when using Zn or Zn compounds as a catalyst can be avoided by further preparation of the surface, for example by deposition of a dielectric layer of material on the substrate, and/or by functionalizing the semiconductor or dielectric surface, e.g. pre-treating the semiconductor or dielectric surface with H 2 S, in other words by for instance sulfidizing the surface before applying ALD.
- a temperature of about 500° C. this leads to a self-limiting reaction resulting in a monolayer coverage of the Si surface with sulphur. Any suitable ALD technique may be applied.
- thermal ALD or plasma enhanced ALD (PEALD) in which the deposition is enforced by plasma (by applying plasma during a unit deposition cycle, for example, applying H 2 X plasma pulse or a mixture of H 2 X and H 2 in a plasma pulse during the second pulse, or applying a H 2 plasma pulse after or during the first pulse, the present invention not being limited thereto).
- plasma by applying plasma during a unit deposition cycle, for example, applying H 2 X plasma pulse or a mixture of H 2 X and H 2 in a plasma pulse during the second pulse, or applying a H 2 plasma pulse after or during the first pulse, the present invention not being limited thereto).
- a method according to embodiments of the present invention may comprise removing the native oxide layer from the substrate before functionalization.
- the surface may include a dielectric layer, for example obtained by deposition via ALD, for example deposition of Si 3 N 4 , SiO 2 , of Al 2 O 3 , or otherwise providing a controlled oxidation of the surface (hence obtaining SiO 2 ).
- the surface may be obtained according any suitable technique, the present invention not being limited thereto.
- the method may include functionalization of the dielectric surface, or directly PEALD.
- Avoiding using Zn may be done by performing thermal ALD directly on a substrate comprising a sacrificial layer.
- the sacrificial monolayer or monolayer stack may be obtained by deposition, for example semiconductor deposition, or deposition of a very thin sacrificial layer or monolayer stack of dielectrics such TiN.
- the thickness of the sacrificial layer for example 2 monolayers or less, may be used to control the deposition (for example, control of the thickness of the ALD layer).
- semiconductor materials suitable for the thin sacrificial layer are Si, GaAs, Ge, or any other semiconductor, the present invention not being limited to these examples.
- the step of functionalization may be omitted in case of deposition of a thin sacrificial layer.
- FIG. 3 illustrates in general steps of a method 300 according to embodiments of the present invention.
- a method according to embodiments of the present invention starts with obtaining 310 a substrate having a surface.
- the substrate can for instance be a semiconductor substrate, a conductive substrate, a dielectric substrate, or a combination thereof.
- the substrate can for instance be an SOI substrate, with a sacrificial layer, for instance a Si layer, or a TiN layer, on top of an insulating layer, for instance an oxide layer.
- the top layer may be a sacrificial layer, in which case functionalization may be omitted, and the step of deposition (using thermal ALD) may be directly applied.
- the substrate can comprise a semiconductor layer, for instance but not limited thereto a Si layer, a Ge layer, a GaAs layer, with a dielectric on top.
- the dielectric on top of the semiconductor layer may for instance be a SiO 2 layer, an Al 2 O 3 layer, or an epitaxially grown mono-crystalline oxide. It is advantageous to use an epitaxially grown oxide, as the lattice constant of such oxide can be tailored so as to have a perfect match with the later on to be provided MX 2 layer.
- an MX 2 layer is deposited on the surface using ALD deposition, for example using thermal ALD, or for example using plasma enhanced ALD in those embodiments not comprising deposition of a sacrificial layer.
- ALD deposition for example using thermal ALD, or for example using plasma enhanced ALD in those embodiments not comprising deposition of a sacrificial layer.
- the number of ALD cycles to be carried out, or the number of sacrificial layers depends on the number of ALD layers to be deposited, typically less than ten in the context of the present invention, where it is desired to obtain thin MX 2 layers.
- a method according to embodiments of the present invention may comprise a further step 330 , where the substrate surface is functionalized.
- the substrate may for instance be sulphidized, i.e. the substrate surface is provided with an S-containing layer. Any suitable method to obtain this may be used.
- a S-containing precursor such as H 2 S is used hereto.
- the substrate may be treated with ozone. Any suitable method to do this may be used.
- the substrate is a semiconductor substrate, such as for instance, but not limited thereto, a silicon substrate.
- FIG. 4 illustrates method steps of a method according to embodiments of the present invention where the substrate is a semiconductor substrate.
- the method comprises a first step 410 of obtaining a semiconductor substrate.
- the semiconductor substrate has a surface.
- native oxide is removed from the semiconductor substrate surface, after which in an optional third step 430 the bare semiconductor substrate is exposed to a functionalization component, e.g. an S-containing component, such as H 2 S, so as to provide the substrate with an S-layer, or ozone.
- a functionalization component e.g. an S-containing component, such as H 2 S
- the S coverage or O coverage may be about one monolayer.
- this functionalization layer is used as a seed layer for providing an MX 2 layer by ALD deposition.
- FIG. 5( a ) to ( d ) show the particular example of how a sulfur layer is built up on a Si surface, after an HF dip and a 5 minutes 850° C. bake in H 2 to remove the last traces of the native oxide, for instance SiO 2 .
- the semiconductor surface would be covered by crystalline oxides, for instance epitaxial, mono-crystalline oxides, which might be composed of SiO x and other oxides, for instance in mixed oxides, there is no need to remove these.
- the semiconductor, e.g. Si, surface is then pretreated by exposure to H 2 S in an inert gas, e.g. N 2 , as carrier gas, at a temperature between 300 and 550° C., and at treatment times of 0.1 to 40 minutes.
- an inert gas e.g. N 2
- the S coverage increases to about a monolayer (as measured with TXRF) after about 10 minutes (cfr FIG. 5( d ) ).
- Cooling down to ALD growth temperature between 100° C. and 400° C., for instance about 300° C., in H 2 results in a —SH coverage of the surface, which is an excellent active site for further ALD growth of the MX 2 material.
- This treatment can e.g. be performed in an ALD reactor with a temperature range up to at least 500° C., or a clustered system in which a substrate can be moved between a reactor for the H 2 S pre-treatment at 500° C. and a more conventional ALD chamber with a temperature range up to at least 350° C.
- Electrons can be captured from an n-type doped semiconductor substrate, e.g. Si substrate, especially in the case where epitaxial seeding from a (111) substrate is used, hence after removal of native oxide. Especially since only very thin MX 2 layers are needed (e.g. typically below 10 monolayers, e.g. up to 7 monolayers, preferably less than 5 monolayers), this is a viable approach.
- a metal halide e.g. MF 6
- MF 6 metal halide
- reaction sequence then could look as follows:
- An alternative initiation procedure for ALD nucleation is to functionalize the semiconductor surface, e.g. Si surface, after native oxide stripping and H 2 -bake for oxygen removal, by using O 3 .
- a semiconductor e.g. Si
- O 3 oxidation e.g. about 40-80° C.
- the Si surface can be functionalized with —OH groups which is an ideal active site for further ALD growth of MX 2 material. It is very likely that these OH groups allow further epitaxial line-up for MX 2 to be grown on top of this, starting with the sulfur layer, with S replacing O.
- This first half cycle then ends up in a Si—O—SH or Si—SH sequence, which then is the starting of the MX 2 layer.
- the (111) Si atomic plane has a unit cell parameter (distance between two neighboring Si atoms) in the order of 3.8 ⁇ .
- An even more interesting surface for epitaxial seeding is an epitaxial layer of wurtzite AlN grown on (111) Si substrates in AlN[0 0 01]//Si[1 1 1] relationship.
- the unit cell parameter a for (0001) AlN is 3.1, which is even closer to the unit cell parameter a of MX2.
- Another good surface can be offered by 4H or 6H SiC, also epitaxially grown on (111) Si.
- the a constant of 4H or 6H SiC is 3.07.
- AlN and SiC are very wide bandgap materials, offering substantial electrical isolation between the MX 2 layer and the (111) Si substrate.
- the resulting product of this process is a stack comprising a predefined number of layers of MX 2 , for example but not limited thereto WS 2 or MoS 2 , whereas a covalent silicon sulfide type of bond is not desired.
- the enthalpy of formation ⁇ H f o of SiS 2 , WS 2 and MoS 2 is resp. ⁇ 34.7, ⁇ 46.3 and ⁇ 61.2 kcal/mole, meaning that SiS 2 is the least stable of these three materials. In view of this, it is not unlikely that the formed MX 2 film can be detached from the Si surface, such as upon thermal annealing, and remains on the surface only by means of van der Waals forces.
- the substrate comprises a dielectric layer at the top.
- the substrate may for instance comprise a semiconductor layer with a dielectric such as Si 3 N 4 , or an oxide layer, e.g. SiO 2 , Al 2 O 3 , HfO 3 , ZrO 2 , or an epitaxially grown oxide on top thereof.
- the optional step of stripping the native oxide from the surface can be omitted if desired.
- a method 600 according to embodiments of the present invention is illustrated in FIG. 6 .
- a substrate having a dielectric top surface e.g. by means of a dielectric layer at its top, is obtained.
- Such dielectric layer can be provided by deposition, or a dielectric layer can be grown atop a semiconductor layer.
- a Si substrate can be oxidized such that a SiO 2 layer atop the Si substrate is formed.
- the obtained substrate can simply be a completely dielectric surface.
- this dielectric substrate or top layer can be functionalized, for example sulphidized, for instance by replacing OH bonds by SH bonds.
- the sulphidizing step may for instance be carried out at a temperature between 300° C. and 500° C., during a time period between about 1 minute and about 1 hour.
- the optional functionalization may be performed with ozone.
- a third reagent from the group of SiH 4 , Si 3 H 8 , Si 2 H 6 , B 2 H 6 may be included, for example as part of a plasma mixture.
- a layer of MX 2 is deposited on the optionally functionalized surface, using ALD deposition.
- the number of ALD cycles applied determines the thickness of the deposited MX 2 layer, which may be limited in the context of the present invention, e.g. less than ten layers, for instance not more than seven layers, not more than five layers, e.g. only one or two layers.
- thermal ALD may be used after sulphidization or functionalization with ozone (for example, after sulphidization or functionalization with ozone of a semiconductor substrate, or after functionalization of a dielectric substrate layer with e.g. SiH 4 , Si 2 H 6 , Si 3 H 8 , B 2 H 6 compounds).
- Thermal ALD may comprise the unit cycle:
- H 2 X pulse e.g. H 2 S pulse
- This sequence is suitable after functionalization or after providing a sacrificial layer.
- the thickness of the sacrificial layer would determine the thickness of the deposited layer.
- the cycle may be repeated a number of times, which would determine the size of the deposition layer.
- the deposition may be performed between e.g. 250 and 450° C.
- the optional functionalization may also comprise SiH 4 , Si 2 H 6 , Si 3 H 8 , B 2 H 6 compounds, in which case plasma can be advantageously used.
- PEALD may advantageously be performed on the dielectric layer, due to the fact that PEALD promotes nucleation on dielectric layers.
- the H 2 (S) plasma may generate H atoms for the chemical reduction of M 6+ . If in the present example a dielectric layer of SiO 2 is used, it can react with MF 6 , binding the F atoms into the volatile SiF 4 or SiHF 3 , thusly initiating the nucleation on the inert dielectric.
- PEALD may be advantageously performed after functionalization comprising silicon-hydrogen compounds, but it may be performed after any other type of functionalization. PEALD may also be performed directly on the substrate, omitting the functionalization. PEALD can be applied following the unit cycle
- Plasma pulse comprising H 2 S, or mixture of H 2 and H 2 X, or mixture of noble gasses with H 2 X
- the PEALD may also be performed according to complex unit cycles (or reaction cycles). Parameters like temperature, pulse time and purge times, number of cycles, and power of pulses may be optimized. Some examples of PEALD reaction cycles are:
- the obtained substrate may include a sacrificial layer on the surface, for instance a semiconductive layer such as a Si layer, or a TiN layer.
- ALD deposition of an MX 2 layer may be performed on such substrate.
- the functionalization may be omitted and the ALD may be directly performed after obtaining the substrate, obtaining a wide deposition area and saving time.
- the initial substrate may comprise a multi-layer structure, for example a semiconductor layer coated with a protective dielectric layer.
- the dielectric layer may be obtained, e.g. deposited, after removing native oxide, for example via H 2 plasma.
- the dielectric layer may comprise for example Si 3 N 4 , or crystalline Al 2 O 3 , or SiO 2 obtained by deposition or by oxidation of the substrate (in case of oxidation, the removal of native oxide may be omitted).
- the dielectric layer is in turn covered by a thin sacrificial monolayer or monolayer stack. In this example, a layer of semiconductor such as Si, Ge, GaAs, or others is applied.
- the sacrificial layer can be obtained by deposition, for example by Molecular Beam Epitaxial (MBE) deposition.
- the thin layer shall ideally comprise one or two monolayers, which could be further protected by addition of a H-passivation layer.
- the thin layer for instance thin Si layer, acts as a solid state reagent during thermal ALD, hence the thickness of the thin layer may be used to control the thickness of the dichalchogenide layer, as the amount of material in the thin layer, e.g. Si, controls the progress of the MF 6 reaction.
- H 2 X will interact so as to bind with the released M 4+ and stabilize it as MX 2 : MF 6 +Si+H 2 X ⁇ MX 2 +SiF 4 +2 HF.
- the compound SiHF 3 may also form in the reaction.
- the thin layer, in the embodiment explained Si layer can be seen as a sacrificial layer or as a solid state redox reagent.
- the ALD sequence in case of the sacrificial Si layer may be a thermal ALD as previously explained, optionally further comprising starting with one or more H 2 X pulses such that H 2 S is present abundantly when MF 6 will attack Si. Nonetheless, the present invention is not limited to a sacrificial layer comprising semiconductor, and the method can be broadened to other materials such as e.g. TiN.
- the present invention provides a method of producing at least two transition metal dichalcogenide materials on a substrate.
- the method comprises the steps of:
- first metal halide precursor is different from the second metal halide precursor and/or the first chalcogen source is different from the second chalcogen source.
- the first and second metals and chalcogenides may be mixed inside the monolayer itself, such as for instance by forming a layer of Mo (1-x) W x S 2(1-y) Se 2y .
- heterogeneous combinations of homogeneous monolayers e.g. MoS 2 on top of WSe 2 may be made.
- metal dichalcogenides e.g. MoS 2 /WS 2
- first layer consisting of a first predefined number N1 of first monolayers (where N1 is an integer value in the range of 1 to 5
- second layer consisting of a second predefined number N2 of second monolayers (where N2 is an integer in the range of 1 to 5
- the stack of all monolayers may be arranged as a lower part of the N1 first monolayers and an upper part of the N2 second monolayers, or as interleaved, e.g. alternating, first and second layers.
- MoF 6 and H 2 S for depositing the first layer, and MoF 6 and H 2 Se for the second layer, or vice versa
- one can make a mixed channel layer MoS 2 /MoSe 2 in well-controlled ratios, e.g. predefined ratios.
- Such a method allows to make semiconductor structures with channels made of different materials in predefined ratios. This allows bandgap engineering of the deposited materials.
- any suitable method according to the present invention for example depositing a protective dielectric layer, a thin sacrificial layer and, via ALD, depositing a first dichalcogenide layer or monolayer stack, then depositing a second thin sacrificial layer and, via ALD, depositing a second dichalcogenide layer or monolayer stack.
- ALD atomic layer deposition
- MX 2 films of monolayer thickness can be deposited by means of ALD starting from MF 6 and H 2 X precursors.
- ALD allows to deposit layers of monolayer thickness with extremely good uniformity, for instance with a standard deviation less than 1% within 1 sigma, at deposition temperatures of 250-450° C., even on large area substrates (e.g. up to 300-450 mm silicon wafers).
- the layer thickness can be controlled to be a predefined number of monolayers (e.g. only one, or only two).
- the procedure may be performed by preparing the surface layer of the substrate and performing ALD.
- the preparation may comprise covering the surface with dielectric, for example comprising SiO 2 , Al 2 O 3 , Si 3 N 4 , a sacrificial layer of TiN, a sacrificial layer of a semiconductor such Si, Ge, GaAs, or others, for instance one or two layers of Si.
- the preparation may also comprise removing the native oxide from the substrate.
- (111) oriented substrates After removing the native oxide, (111) oriented substrates, or an epitaxial layer of wurtzite AlN grown on (111) oriented substrates in AlN[0 0 01]//Si[1 1 1] relationship, or 4H or 6H SiC, also epitaxially grown on a (111) substrate allow to control the orientation of the MX 2 by epitaxial seeding with the basal plane being substantially parallel to the surface.
- the semiconductor surface can be pre-functionalized, e.g. pre-sulphidized by annealing the substrate, either after deposition of the protective layer, or after native oxide removal, in H 2 S at T of about 400° C.
- the reduction of the W 6+ precursor can follow a few different pathways: i) by uptake of electrons from an n-type doped Si substrate; ii) by applying a H 2 plasma such that active H radicals can interact in the chemistry and reduce the W 6+ , or iii) by addition of Si 2 H 6 as a strong reducing agent.
- This avoids the need for a catalyst during the ALD initiation and hence helps preserving a high purity film, e.g. having Zn and C impurities below 1e18/cm 3 .
- ALD may also be directly performed on the sacrificial layer, whose thickness may control the reaction and formation of the TMD layers.
- the functionalization step may be omitted before thermal ALD.
- a method according to embodiments of the present invention allows to produce semiconductor devices with extremely small dimensions. Such devices are particularly suited for continued scaling beyond Si CMOS technology nodes (e.g. beyond the 12 nm technology node).
- the stack of monolayers of MX 2 materials may e.g. be used as alternative transistor channel material for regular MOSFET devices in low-power CMOS, or as material for heterostructures such as used in tunneling devices (TFET), or as material for spintronics.
- TFET tunneling devices
- Such devices may have in particular the following advantages:
- the method described above may also be particularly suited for producing optoelectronic devices requiring transparent semiconductors.
- Transparent material allows use as driving circuits for OLEDs, or as tunable band gap (e.g. by alloys) enables LED.
- the method described above may also be particularly suited for producing electronics on flexible substrates, e.g. wearable electronics, e-newspaper, etc.
- the method described above may also be particularly suited for producing gas sensing devices because they exhibit a highly selective response to electron donors (higher selectivity than CNT sensors), and have quick response times.
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Abstract
Description
-
- It is obtained from best known materials with regard to properties and synthesis (e.g. from catalysis research, lubricants, etc.)
- It has high thermal conductivity which is always good in devices with high transistor density
- Sulfides are expected to have a higher critical electrical field (at which the behavior changes from semiconductor to metal)
-
- a single MoS2 monolayer in combination with a single WS2 monolayer, or
- a single MoS2 monolayer in combination with a double WS2 monolayer, or
- a double MoS2 monolayer in combination with a single WS2 monolayer, or
- a double MoS2 monolayer in combination with a double WS2 monolayer.
2*+H2X→XH+H a.
XH+WF6→XWFx+HF b.
with * denoting an active surface site and XH an XH group connected to a surface site.
HF is an extremely effective leaving group. As such, these precursors allow growth of very pure MX2 films without substantial contamination such as e.g. by carbon, which can be found when using metalorganic precursors. It is known that this ALD sequence has difficulties in nucleating on semiconductor material such as silicon or on a dielectric such as SiO2, and in the prior art the catalytic effect of DEZn (di-ethyl zinc) is used to solve that problem. This, however causes contamination of the MX2 layer by undesired co-deposition of Zn.
(ii) By applying a H2 plasma, reactive H radicals can interact with a metal halide (e.g. MF6) in the chemistry as follows: MF6+H→MH5+HF; MF5+H→MH4+HF. In this way, H goes into a redox reaction with MF6 resulting in the formation of HF and the reduction of the M6+. In view of the low deposition temperature (e.g. less than 500° C.), it is unlikely that H2 can initiate similar reactions (due to the thermal stability of H2).
(iii) By adding a third reagent, i.e. Si2H6, which is a strong reducing agent, according to the overall reaction: WF6+Si2H6→W+2SiHF3+2H2. This reaction is the basis of W ALD such as used for deposition of W contacts and vias in mainstream Si CMOS technology. A detailed description of W ALd using WF6 and Si2H6 can be found in J. W. Elam, C. E Nelson, R. K. Grubbs and S. M. George, Kinetics of the WF6 and Si2H6 surface reactions during tungsten atomic layer deposition, Surface Science 479 (2001) 121-135. In this reaction, Si from the Si2H6 molecule reacts with WF6 to remove sequentially the F ions. Simultaneously, the H1− (hydride) ions from Si2H6 are converted to H0 in H2, which is the oxidation part of the redox system. In the case of embodiments of the present invention, however, different from the W ALD case, the reduction of WF6 to W is stopped at the intermediate state of W4+ due to the bonding with S at the stage of WS4, since WS4 is a more stable compound than W in these conditions. Due to the strong atomic Si—F bond, contamination by Si is not likely as SiHF3 is a volatile reaction by-product and will be exhausted readily. Similar reaction schemes can be thought of for the other transitions metals as well as for the Se case.
- 1. Providing a substrate and a surface
- 2. Providing a sulphur surface layer from H2S treatment at appropriate temperature
- 3. Injecting consequentially WF6, Si2H6, and H2S in well-separated pulses including inert gas purges in between the pulses
-
- Metal halide and H2 plasma cyclically, followed by pulse of H2S.
- Metal halide precursor pulse, followed by cycles of H2 plasma and H2S
- Metal halide precursor pulse, followed by cycles of H2S and H2 plasma
- Cycles of metal halide and H2S, followed by a pulse of H2 plasma
- Cycles of metal halide and H2 plasma, followed by cycles of H2S and H2 plasma
Purging can be done after or during a reaction cycle.
-
- a single MoS2 monolayer in combination with a single WS2 monolayer, or
- a single MoS2 monolayer in combination with a double WS2 monolayer, or
- a double MoS2 monolayer in combination with a single WS2 monolayer, or
- a double MoS2 monolayer in combination with a double WS2 monolayer.
-
- high ION/IOFF ratio, providing low power consumption in the OFF-state,
- low subtreshold voltage swing, hence suitable for low voltage operation,
- lower dielectric constant than Silicon resulting in a smaller characteristic length, and therefore no short channel effects expected at small gate lengths,
- low dimensional material (thickness of 1 monolayer of about 0.68 nm), hence ultra-thin body,
- MoS2 layers (basal planes) are believed to be chemically inert due to the sulfur termination. In contrast, the edges of patterned MX2 are highly active due to the dangling bonds at these edges;
Claims (19)
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PCT/EP2014/078441 WO2015091781A2 (en) | 2013-12-18 | 2014-12-18 | Method of producing transition metal dichalcogenide layer |
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US20170250075A1 (en) | 2017-08-31 |
WO2015091781A3 (en) | 2015-08-27 |
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